CN108841190A - A kind of preparation method of degradable plastic film - Google Patents
A kind of preparation method of degradable plastic film Download PDFInfo
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- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
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Abstract
The present invention relates to a kind of preparation methods of degradable plastic film, belong to degradation material technical field.What the present invention selected is cotton stalk and orange peel, cost is very cheap, the cellulose contained by cotton stalk has good degradability and biocompatibility, while the good mechanical performance of cellulose simultaneously, can make up for it the poor disadvantage of the universal mechanical performance of degradable plastic film；The shortcomings that orange peel pectin content is abundant, can increase the degree of adhesion between each material, while mechanical strength also can be enhanced, and pectin all has stability to heat and acid, can make up for it common degradation material poor heat resistance；Degradable plastic film water resistance and acid resistance of the present invention are all relatively good, and there is better mechanical performance than common degradable plastic film, and simple production process, the raw materials for production used are degradable and low in cost, can be widely applied to degradable plastic film manufacturing field.
Description
Technical field
The present invention relates to a kind of preparation methods of degradable plastic film, belong to degradation material technical field.
Background technique
Plastic products have the advantages that stability is strong, light, production cost is low etc., thus the deep pro-gaze by people.Nearly tens
Plastics industry is grown rapidly over year, the use of a large amount of plastic products especially Phthalates, to the life of the mankind
It brings great convenience.It, can be long-term in the environment after its abandoned but due to the chemical stability of general-purpose plastics itself
It is stabilized, causes the accumulation of a large amount of plastic refuses in the environment, serious harm is brought to environment, such as white pollution, agriculture
The problems such as industry white cancer.
Other than white pollution, to ecological environment, there is also potentially hazardous for they.（1）Harm to agricultural：By
In the air impermeability and waterproofness of plastics, after mixing together with soil, absorption of the crops to nutrient, moisture just will affect, from
And lead to crop production reduction；（2）Threat to animal survival：Animal is in the plastic package foods that phagocytosis is abandoned by the mankind, modeling
Material packaging film is often swallowed together, and the plastics accidentally swallowed are detained for a long time in the stomach of animal to be difficult to digest, and is eventually led to
Animal dead；（3）Influence the sustainable use in soil：Plastic quality is light, volume is big, in the soil with garbage loading embeading, the centuries
It will not all change, seriously affect soil texture, and long-term land occupation resource.
With the continuous improvement of environmental problem to become increasingly conspicuous and human environment protection is realized, the place of plastic refuse
Reason problem has become the focus of international community's extensive concern.It solves the problems, such as that this method mainly has incineration method at present, fills
Method and recycling etc..
Incineration method is one of main method for the treatment of of urban garbage, and plastic refuse has a high fuel value, and when burning can
To discharge a large amount of heat, therefore burning with higher is worth.Landfill method is the most widely used side of domestic and international processing rubbish
Method is broadly divided into two classes at present：Traditional landfill method and sanitary landfill method.Recycling and reusing is that the plastic refuse that will be recycled passes through
The processes such as classification, broken, cleaning, are then processed by dedicated Granulation Equipments, to obtain the master batch of regenerated plastics, make to provide
Source obtains cycling and reutilization.
The above several method is still the common method of numerous national disposal of plastic waste at present, as what is be individually present asks
Topic becomes increasingly conspicuous, and above-mentioned several method is no longer satisfied requirement of the mankind to environmental protection.Fundamentally solve plastic waste
New problem solution route is sought in gurry pollution problem, is the highly desirable realization of the mankind.It, can be with after degradation plastic is discarded
It is degraded using certain factors in environment, so the accumulation of plastic refuse in the environment can be reduced, and then from basic
The upper pollution problem for solving plastic refuse to environment.Therefore, develop degradation plastic and have become solution plastic refuse dirt
The final approach of dye problem.
Summary of the invention
The technical problems to be solved by the invention：It is at high cost for the degradation plastic that produces at present, mechanical strength is lower
The problem of, provide a kind of preparation method of degradable plastic film.
In order to solve the above technical problems, the technical solution adopted by the present invention is that：
（1）Sodium hydroxide is added after cotton stalk is shredded and deionized water is boiled, stops heating after 2~3h, stands cooling, to
When temperature is cooled to 70~80 DEG C, hydrogen peroxide is added, continues to heat 0.5h, temperature is maintained at 70~80 DEG C；
（2）Filter residue and drying is obtained stalk fibre by filter mixed liquor；
（3）0.1mol/L hydrochloric acid is added after orange peel is shredded to boil, stirs, is filtered after 2~3h simultaneously, collect filtrate；
（4）Active carbon is added in filtrate, is heated to 50~60 DEG C, dehydrated alcohol is added after 30min and is stood, must be flocculated out
Pectin and drying and crushing obtain dry pectin；
（5）By nano silica, polyacrylamide and deionized water high-speed stirred, nanometer titanium dioxide silicon emulsion is obtained；
（6）By nanometer titanium dioxide silicon emulsion, stalk fibre, dry pectin, polylactic acid, polyethylene succinate, plasticizer and heat
Stabilizer is put into high-speed mixer stirring, obtains masterbatch；
（7）Masterbatch is put into filling twin-screw extrusion master batch, then master batch is put into inflation film manufacturing machine, Blown Film simultaneously cuts winding,
Degradable plastic film can be obtained.
Step（1）The cotton stalk, sodium hydroxide, deionized water and hydrogen peroxide mass ratio be 500：5：1000：10.
Step（3）The mass ratio of the orange peel and hydrochloric acid is 500：1000, the temperature boiled is 100 DEG C.
Step（4）The mass ratio of the active carbon, filtrate and dehydrated alcohol is 200：1：400.
Step（5）The mass ratio of the nano silica, polyacrylamide and deionized water is 100：1：400.
Step（6）The stalk fibre dries pectin, polylactic acid, polyethylene succinate, plasticizer and heat stabilizer
Mass ratio is 200：50：50：50：20：10.
Step（6）The plasticizer is any one in acetyl tri-n-butyl citrate or tri-n-butyl citrate.
Step（6）The heat stabilizer is any one in calcium stearate or zinc stearate.
The present invention is compared with other methods, and advantageous effects are：
（1）What the present invention selected is cotton stalk and orange peel, and cost is very cheap, while the cellulose contained by cotton stalk
With good degradability and biocompatibility, while the good mechanical performance of cellulose, it is thin to can make up for it degradation plastic
The poor disadvantage of the universal mechanical performance of film；
（2）Orange peel is extremely easy to get, and pectin content is abundant, and pectin can increase the degree of adhesion between each material,
Mechanical strength also can be enhanced simultaneously, and pectin all has stability to heat and acid, and it is resistance to can make up for it common degradation material
The disadvantage of hot difference；
（3）Stalk fibre that the present invention uses, pectin, polylactic acid, polyethylene succinate, plasticizer are all degradable materials
Material, simultaneously because the pectin of addition has thermal stability, it is possible to reduce the input amount of heat stabilizer further enhances degradable
Property；
（4）Nano silica due to size is small, large specific surface area, surface can high, surface exist a large amount of unsaturated residual bonds and
The hydroxyl of different bond styles can be improved intermolecular bonding force, while is easily distributed in the gap of macromolecular chain again, with big point
Son is combined with each other as solid netted, to increase substantially film strength, elasticity and water resistance, nano silica is passed through
After high-speed stirred is evenly dispersed, the coarse structure on producing fibre from cotton stalk surface provides attachment point for nano silica, and
The addition of pectin is so that producing fibre from cotton stalk, nano silica, polylactic acid and polyethylene succinate connect even closer, increasing
Strong mechanical performance；
（5）Degradable plastic film water resistance and acid resistance of the present invention are all relatively good, and than common degradable plastic film
With better mechanical performance, and simple production process, the raw materials for production used are degradable and low in cost, can answer extensively
For degradable plastic film manufacturing field.
Specific embodiment
500~600g cotton stalk is shredded, 5~10g sodium hydroxide and 1000~1200g deionization boiling is then added
After boiling 2~3h, cooling is stood, when solution temperature is down to 70~80 DEG C, 10~20g hydrogen peroxide is added, continues to heat 0.5h,
70~80 DEG C are maintained the temperature at, filters and washs filter residue later, obtain stalk fibre after dry；Take 500~600g orange peel
Chopping is added the hydrochloric acid solution boiling of 1000~1200g0.1mol/L, stirs in boiling, filter after 2~3h, collects filtrate；
It takes 200 ~ 300g filtrate that 1 ~ 2g active carbon is added, is heated to 50~60 DEG C, 400~600g dehydrated alcohol is added after 30min, stand
After 30min, the pectin and drying and crushing that must be flocculated out obtain dry pectin；100~150g nano silica, 1~1.5g are poly-
Acrylamide and 400~600g deionized water, 0.5~1h of high-speed stirred obtain nanometer titanium dioxide silicon emulsion；40~60g is received
Rice silica lotion, 200~300g stalk fibre, 50~75g dry pectin, 50~75g polylactic acid, 50~75g polyethylene
Succinate, 20~30g plasticizer and 10~15g heat stabilizer are put into high-speed mixer and stir 2~3h, obtain masterbatch；It will be female
Master batch is squeezed out in material filling double screw extruder, then master batch is put into inflation film manufacturing machine, Blown Film simultaneously cuts winding, can be obtained
Degradable plastic film.
Example 1
500g cotton stalk is shredded, after then addition 5g sodium hydroxide and 1000g deionized water boil 2h, stands cooling, to
When solution temperature is down to 70 DEG C, 10g hydrogen peroxide is added, continues to heat 0.5h, maintains the temperature at 70 DEG C, filter and wash later
Filter residue obtains stalk fibre after dry；It takes 500g orange peel to shred, the hydrochloric acid solution boiling of 1000g0.1mol/L, side is added
Boiling side is stirred, and is filtered after 2h, and filtrate is collected；200g filtrate is taken, 1g active carbon is added, is heated to 50 DEG C, is added after 30min
400g dehydrated alcohol, after standing 30min, the pectin and drying and crushing that must be flocculated out obtain dry pectin；100g nanometer titanium dioxide
Silicon, 1g polyacrylamide and 400g deionized water, high-speed stirred 0.5h obtain nanometer titanium dioxide silicon emulsion；By 40g nano-silica
The dry pectin of SiClx lotion, 200g stalk fibre, 50g, 50g polylactic acid, 50g polyethylene succinate, 20g plasticizer and 10g
Heat stabilizer is put into high-speed mixer stirring 2h, obtains masterbatch；Masterbatch is inserted in double screw extruder and squeezes out master batch, then will be female
Grain is put into inflation film manufacturing machine, and Blown Film simultaneously cuts winding, and degradable plastic film can be obtained.
Example 2
550g cotton stalk is shredded, after then addition 8g sodium hydroxide and 1100g deionized water boil 2h, stands cooling, to
When solution temperature is down to 75 DEG C, 15g hydrogen peroxide is added, continues to heat 0.5h, maintains the temperature at 75 DEG C, filter and wash later
Filter residue obtains stalk fibre after dry；It takes 550g orange peel to shred, the hydrochloric acid solution boiling of 1100g0.1mol/L, side is added
Boiling side is stirred, and is filtered after 2h, and filtrate is collected；250g filtrate is taken, 1g active carbon is added, is heated to 55 DEG C, is added after 30min
500g dehydrated alcohol, after standing 30min, the pectin and drying and crushing that must be flocculated out obtain dry pectin；125g nanometer titanium dioxide
Silicon, 1.2g polyacrylamide and 500g deionized water, high-speed stirred 0.8h obtain nanometer titanium dioxide silicon emulsion；By 50g nanometer two
Aoxidize the dry pectin of silicon emulsion, 250g stalk fibre, 65g, 65g polylactic acid, 65g polyethylene succinate, 25g plasticizer and
12g heat stabilizer is put into high-speed mixer stirring 2h, obtains masterbatch；Masterbatch is inserted in double screw extruder and squeezes out master batch, then
Master batch is put into inflation film manufacturing machine, Blown Film simultaneously cuts winding, and degradable plastic film can be obtained.
Example 3
600g cotton stalk is shredded, after then addition 10g sodium hydroxide and 1200g deionized water boil 3h, stands cooling, to
When solution temperature is down to 80 DEG C, 20g hydrogen peroxide is added, continues to heat 0.5h, maintains the temperature at 80 DEG C, filter and wash later
Filter residue obtains stalk fibre after dry；It takes 600g orange peel to shred, the hydrochloric acid solution boiling of 1200g0.1mol/L, side is added
Boiling side is stirred, and is filtered after 3h, and filtrate is collected；300g filtrate is taken, 2g active carbon is added, is heated to 60 DEG C, is added after 30min
600g dehydrated alcohol, after standing 30min, the pectin and drying and crushing that must be flocculated out obtain dry pectin；150g nanometer titanium dioxide
Silicon, 1.5g polyacrylamide and 600g deionized water, high-speed stirred 1h obtain nanometer titanium dioxide silicon emulsion；By 60g nano-silica
The dry pectin of SiClx lotion, 300g stalk fibre, 75g, 75g polylactic acid, 75g polyethylene succinate, 30g plasticizer and 15g
Heat stabilizer is put into high-speed mixer stirring 3h, obtains masterbatch；Masterbatch is inserted in double screw extruder and squeezes out master batch, then will be female
Grain is put into inflation film manufacturing machine, and Blown Film simultaneously cuts winding, and degradable plastic film can be obtained.
Reference examples：The degradable plastic film of Zhejiang company production.
The degradable plastic film of example and reference examples is detected, specific detection is as follows：
Thermal-oxidative degradation performance：Film similar in size is put into electric heating constant-temperature blowing drying box simultaneously, and is separated with partition, mould
Quasi- compost temperature, sets heating temperature as 70 DEG C.Separated in time takes out, and each sample clip sample segment is analyzed
Characterization.It is stored in refrigerator before samples taken analysis test, prevents sample further occurrence thermal oxidative degradation.
Biodegrade：According to standard GB/T1927.6.2-2003/ISO14852：1999《Material is final in aqueous medium
The measurement of aerobic biodegradability ability discharges the method for carbon dioxide using measurement》It is tested.
Photooxidation droping：Experimental thin films are cut into 3cm × 10cm respectively, and choose film similar in quality, are placed in quartzy glass
In glass test tube, it is placed in roof in 45 degree of angles with ground, sunlight light irradiates under natural conditions.It is spaced same time to take out, go forward side by side
Row is analyzed and characterized.
Specific testing result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Thermal-oxidative degradation % | 34.71 | 30.51 | 31.52 | 20.91 |
| Biodegradable % | 13.86 | 15.26 | 14.36 | 5.47 |
| Photooxidation droping % | 35 | 30 | 32 | 20 |
As shown in Table 1, degradable plastic film prepared by the present invention improves the light degradation effect and thermal degradation effect of film, together
When improve the biological decomposition rate of film, therefore, be with a wide range of applications as a kind of novel degradation plastic.
Claims (8)
1. a kind of preparation method of degradable plastic film, which is characterized in that specifically preparation step is：
（1）Sodium hydroxide is added after cotton stalk is shredded and deionized water is boiled, stops heating after 2~3h, it is cooling to temperature
When to 70~80 DEG C, hydrogen peroxide is added, continues to heat 0.5h, temperature is maintained at 70~80 DEG C；
（2）Filter residue and drying is obtained stalk fibre by filter mixed liquor；
（3）0.1mol/L salt acid cooking is added after orange peel is shredded, stirs, is filtered after 2~3h simultaneously, collects filtrate；
（4）Active carbon is added in filtrate, is heated to 50~60 DEG C, dehydrated alcohol is added after 30min and is stood, must be flocculated out
Pectin and drying and crushing obtain dry pectin；
（5）By nano silica, polyacrylamide and deionized water high-speed stirred, nanometer titanium dioxide silicon emulsion is obtained；
（6）By nanometer titanium dioxide silicon emulsion, stalk fibre, dry pectin, polylactic acid, polyethylene succinate, plasticizer and heat
Stabilizer is put into high-speed mixer stirring, obtains masterbatch；
（7）Masterbatch is put into filling twin-screw extrusion master batch, then master batch is put into inflation film manufacturing machine, Blown Film simultaneously cuts winding,
Degradable plastic film can be obtained.
2. a kind of preparation method of degradable plastic film as described in claim 1, which is characterized in that step（1）The cotton
Chopped straw stalk, sodium hydroxide, deionized water and hydrogen peroxide mass ratio be 500：5：1000：10.
3. a kind of preparation method of degradable plastic film as described in claim 1, which is characterized in that step（3）The tangerine
The mass ratio of sub- skin and hydrochloric acid is 500：1000, the temperature boiled is 100 DEG C.
4. a kind of preparation method of degradable plastic film as described in claim 1, which is characterized in that step（4）The work
Property charcoal, filtrate and dehydrated alcohol mass ratio be 200：1：400.
5. a kind of preparation method of degradable plastic film as described in claim 1, which is characterized in that step（5）It is described to receive
The mass ratio of rice silica, polyacrylamide and deionized water is 100：1：400.
6. a kind of preparation method of degradable plastic film as described in claim 1, which is characterized in that step（6）The straw
Stalk fiber, the mass ratio for drying pectin, polylactic acid, polyethylene succinate, plasticizer and heat stabilizer are 200：50：50：50：
20：10.
7. a kind of preparation method of degradable plastic film as described in claim 1, which is characterized in that step（6）The increasing
Agent is moulded as any one in acetyl tri-n-butyl citrate or tri-n-butyl citrate.
8. a kind of preparation method of degradable plastic film as described in claim 1, which is characterized in that step（6）The heat
Stabilizer is any one in calcium stearate or zinc stearate.
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